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Sodium Carbonate → Methyl 4-[4-[([1,1'-biphenyl]-2-ylcarbonyl)amino]phenyl]-alpha-phenyl-1-piperazineacetate

HRID 1804437
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인쇄 미리보기

반응식

HRID 1804437 반응식
Br[CH:2]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:3]([O:5][CH3:6])=[O:4].[N:13]1([C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26]([C:28]3[C:29]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)=[CH:30][CH:31]=[CH:32][CH:33]=3)=[O:27])=[CH:21][CH:20]=2)[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C>[C:29]1([C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=1[C:26]([NH:25][C:22]1[CH:21]=[CH:20][C:19]([N:13]2[CH2:18][CH2:17][N:16]([CH:2]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)[C:3]([O:5][CH3:6])=[O:4])[CH2:15][CH2:14]2)=[CH:24][CH:23]=1)=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 137806Benzeneacetic acid, alpha-bromo-, methyl esterHCID 22499369N-[4-(1-piperazinyl)phenyl]-[1,1'-biphenyl]-2-carboxamide

생성물 1

HCID 22499399Methyl 4-[4-[([1,1'-biphenyl]-2-ylcarbonyl)amino]phenyl]-alpha-phenyl-1-piperazineacetate수율 85.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

Methyl α-bromo-α-phenylacetate (0.1 mole) was added dropwise to a stirring mixture of intermediate (10) (0.07 mole) and Na2CO3 (13 g) in DMF (300 ml). The mixture was stirred overnight. The solvent was evaporated. The residue was crystallized from methanol. The precipitate was filtered off and dried, yielding 30.2 g of methyl 4-[4-[([1,1′-biphenyl]-2-ylcarbonyl)amino]phenyl]-α-phenyl-1-piperazineacetate (melting point 125° C.) identified as compound No. 52 in the following table F-1.

후처리

  1. customThe solvent was evaporated
  2. customThe residue was crystallized from methanol
  3. filtrationThe precipitate was filtered off
  4. customdried

출처 및 근거

ORD 기록
ord-9a56f5782fe144caa4993f2f9cb901b6
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354402B2

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